EP0212940A2 - Verfahren zur Herstellung einer Graphiteinlagerungsverbindung - Google Patents
Verfahren zur Herstellung einer Graphiteinlagerungsverbindung Download PDFInfo
- Publication number
- EP0212940A2 EP0212940A2 EP86306249A EP86306249A EP0212940A2 EP 0212940 A2 EP0212940 A2 EP 0212940A2 EP 86306249 A EP86306249 A EP 86306249A EP 86306249 A EP86306249 A EP 86306249A EP 0212940 A2 EP0212940 A2 EP 0212940A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- chloride
- reaction
- graphite
- metal chloride
- metal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 74
- 239000010439 graphite Substances 0.000 title claims abstract description 74
- 230000002687 intercalation Effects 0.000 title claims abstract description 55
- 238000009830 intercalation Methods 0.000 title claims abstract description 55
- 150000001875 compounds Chemical class 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims description 18
- 238000002360 preparation method Methods 0.000 title claims 3
- 238000006243 chemical reaction Methods 0.000 claims abstract description 66
- 229910001510 metal chloride Inorganic materials 0.000 claims abstract description 49
- 238000009835 boiling Methods 0.000 claims abstract description 10
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims abstract description 9
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 30
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 30
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 17
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 17
- 229960003280 cupric chloride Drugs 0.000 claims description 15
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 12
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 12
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 8
- 229910021555 Chromium Chloride Inorganic materials 0.000 claims description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 2
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 claims description 2
- 229940099607 manganese chloride Drugs 0.000 claims description 2
- 235000002867 manganese chloride Nutrition 0.000 claims description 2
- 239000011565 manganese chloride Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 16
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 15
- 239000000460 chlorine Substances 0.000 abstract description 15
- 229910052801 chlorine Inorganic materials 0.000 abstract description 15
- 230000035484 reaction time Effects 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 description 12
- 230000001965 increasing effect Effects 0.000 description 7
- 229910021382 natural graphite Inorganic materials 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000003780 insertion Methods 0.000 description 5
- 230000037431 insertion Effects 0.000 description 5
- 230000002194 synthesizing effect Effects 0.000 description 5
- 238000012790 confirmation Methods 0.000 description 4
- -1 for example Chemical class 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910021630 Antimony pentafluoride Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- VBVBHWZYQGJZLR-UHFFFAOYSA-I antimony pentafluoride Chemical compound F[Sb](F)(F)(F)F VBVBHWZYQGJZLR-UHFFFAOYSA-I 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/22—Intercalation
Definitions
- This invention relates to a method for the production of a graphite intercalation compound. More particularly, this invention relates to a method for the production of a graphite intercalation compound which, by effecting the reaction for the production in the presence of a second metal chloride besides the metal chloride destined to form the intercalant aimed at, notably shortens the time required for the synthesis of the graphite intercalation compound and permits the synthesis to be carried out effectively without using chlorine.
- the graphite intercalation compounds have been found to combine the chemical stability inherent in graphite and other properties with high degrees of electroconductivity proper to metals. The knowledge has encouraged numerous researches. These researches have unveiled the fact that graphite intercalation compounds have their nature governed by the kinds of intercalants inserted therein.
- the graphite intercalation compound which has an alkali metal such as, for example, potassium as an intercalant
- the graphite intercalation compound lacks stability in the air and yields to decomposition, though it enjoys improved electroconductivity (Y. Iye et al., Phys. Rev. B, 25, 4583, 1982).
- the graphite intercalation compounds using metal chlorides as their intercalants possess degrees of electroconductivity that fall short of that of copper metal but compare favorably with those of almost all metals and, what is more, enjoy stability in the air.
- the graphite intercalation compound is stable not only in the air but also under water.
- the reaction for the intercalation of cupric chloride into graphite proceeds so slowly that some tens of days are required for completion of the reaction (Takahashi et al., Glossary of Lectures for the llth Annual Meeting of The Carbon Society of Japan, page 42, 1984). Owing to the slowness of the reaction, quantity use of the compound has proved virtually impracticable.
- the inventors have continued a diligent study for the purpose of solving the problems and notably increasing the velocity of the reaction. They have consequently found that the velocity of the reaction can be heightened by allowing a second metal chloride of a low boiling point to be present in a minute amount in the reaction system and that the presence of the minute amount of the second metal chloride of a low boiling point enables the reaction for which the presence of chlorine gas has been found an indispensable requirement to proceed to completion in the absence of chlorine gas.
- the present invention has been perfected as the result.
- a metal chloride such as, for example, ferric chloride, cupric chloride, nickel chloride, aluminum chloride, or cobalt chloride
- a specific metal chloride such as, for example, nickel chloride
- this invention aims to provide a method which is characterized by allowing the reaction for the production to proceed in the presence, besides the metal chloride intended for the intercalation, of a second chloride having a realtively low boiling point and in the absence of chlorine gas.
- a metal chloride such as, for example, ferric chloride, cupric chloride, aluminum chloride, nickel chloride, cobalt chloride, manganese chloride, or chromium chloride
- a metal chloride such as, for example, ferric chloride, cupric chloride, aluminum chloride, nickel chloride, cobalt chloride, manganese chloride, or chromium chloride
- a second metal chloride of a relatively low boiling point such as, for example, ferric chloride (boiling point, 317°C), aluminum chloride (sublimation point 183°C), cupric chloride, or cobalt chloride and, in the production of a graphite intercalation compound using a specific metal chloride such as, for example, nickel chloride previously held capable of inducing successful synthesis of the compound only under an atmosphere of chlorine, obviates necessity for use of chlorine by the use of a minute amount of the second metal chloride.
- a specific metal chloride such as, for example, nickel chloride previously held
- Preferred metal chlorides which have relatively low boiling points and are usable as said second metal chloride comprise those which have boiling points or sublimation points of not more than 320°C as described above, and those which have higher vapor pressures at the reaction temperature than the vapor pressures that the intercalants have.
- the production of a graphite intercalation compound in accordance with this invention may be attained by charging a reaction vessel with graphite, a metal chloride intended as an intercalant, and a minute amount of a second metal chloride as an additive, vacuumizing the reaction vessel, and sealing it tightly, and allowing the contens thereof to react.
- Any of the various kinds of graphite known to produce graphite intercalation compounds can be used as the graphite for the sake of the reaction.
- Powdery natural graphite, sheetlike natural graphite, sheetlike swelled graphite, graphite fibers, and man-made graphite are examples.
- the amount of the second metal chloride to be added may be in the range of 0.1 to 2.0 % by weight, preferably 0.3 to 2.0% by weight, based on the metal chloride intended as an intercalant. If the second metal chloride is added in an amount exceeding the upper limit of the aforementioned range, there is the possibility that the pressure inside the reaction vessel will rise so much as to jeopardize the safety of the reaction and the second metal chloride will mingle in a large amount in the product and render the control of characteristics such as, for example, thermal stability and electroconductivity difficult. If the amount of the second metal chloride to be added is less than the lower limit of the aforementioned range, the velocity of the reaction is not heightened so much as expected.
- the reaction vessel charged with the raw materials described above may be heated to a temperature in the range of 200°C to 700°C , though variable with the particular kind of metal chloride intended for intercalation, to induce reaction of the raw materials and give rise to the graphite intercalation compound aimed at.
- the addition of a minute amount of a metal chloride other than the metal chloride intended for intercalation between graphite layers is recognized to bring about a notable increase in the velocity of the reaction.
- the exact mechanism responsible for the acceleration of the reaction remains yet to be elucidated.
- the accelerated reaction velocity may be logically explained by a postulate that when the added metal chloride of a relatively low boiling point such as, for example, ferric chloride or aluminum chloride is inserted into the graphite layers or when the chlorine generated in consequence of thermodynamic equilibrium is incorporated between the graphite layers in the initial stage of reaction, it confers electric charge upon the graphite layers and consequently activates the reaction for the intercalation of the metal chloride between the layers; and that the added metal chloride partly forms a metal chloride complex and consequently increases the apparent gaseous partial pressure of the metal chloride intended for intercalation between graphite layers.
- a relatively low boiling point such as, for example, ferric chloride or aluminum chloride
- This invention in the production of a graphite inter- calatin compound using a metal chloride as an intercalant, provides a method of production which permits a notable reduction in the reaction time heretofore protracted so much as to raise a problem. Further, in the production of a graphite intercalation compound using as an intercalant thereof a specific metal chloride capable of inducing the synthesis of the compound only under an atmosphere of chlorine, this invention obviates the necessity for use of chlorine gas owing to the addition of a second metal chloride. Thus, this invention decreases the heating time required during the course of the reaction and brings about an effect of saving energy consumption. Since it permits synthesis of the graphite intercalation compound without use of chlorine, a highly corrosive gas, it contributes to improving the work environment.
- graphite intercalation compounds may be of light weight, good electroconductivity proper to metals, and highly stable in air; and have many uses such as for a light leading wire, EMI shield materials, electroconductive paint, packings, compound, etc..
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP180046/85 | 1985-08-17 | ||
JP60180046A JPS6241706A (ja) | 1985-08-17 | 1985-08-17 | 黒鉛層間化合物の製造方法 |
Publications (3)
Publication Number | Publication Date |
---|---|
EP0212940A2 true EP0212940A2 (de) | 1987-03-04 |
EP0212940A3 EP0212940A3 (en) | 1988-03-16 |
EP0212940B1 EP0212940B1 (de) | 1991-03-27 |
Family
ID=16076537
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP86306249A Expired - Lifetime EP0212940B1 (de) | 1985-08-17 | 1986-08-13 | Verfahren zur Herstellung einer Graphiteinlagerungsverbindung |
Country Status (4)
Country | Link |
---|---|
US (1) | US4729884A (de) |
EP (1) | EP0212940B1 (de) |
JP (1) | JPS6241706A (de) |
DE (1) | DE3678360D1 (de) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0311298A2 (de) * | 1987-10-06 | 1989-04-12 | Cabotex Co. Ltd. | Verfahren zur Bereitung einer Einlagerungsverbindung Bereitung einer Einlagerungsverbindung |
EP0578887A1 (de) * | 1992-07-17 | 1994-01-19 | Inland Steel Company | Verfahren zur Herstellung von Einlagerungsverbindungen |
DE102021207914A1 (de) | 2020-12-15 | 2022-06-15 | Robert Bosch Gesellschaft mit beschränkter Haftung | Verfahren zum Herstellen eines elektrisch leitfähigen Leiterstrangs mit zumindest einem Kohlenstoffleiter |
WO2022128495A1 (de) | 2020-12-15 | 2022-06-23 | Robert Bosch Gmbh | Verfahren zum herstellen eines elektrisch leitfähigen leiterstrangs mit zumindest einem kohlenstoffleiter |
Families Citing this family (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS62138315A (ja) * | 1985-12-10 | 1987-06-22 | Fuji Carbon Seizosho:Kk | 金属塩化物と黒鉛とからなる層間化合物の製造方法 |
JPS62265112A (ja) * | 1986-05-13 | 1987-11-18 | Nippon Steel Corp | 黒鉛層間化合物の製造方法 |
US4837377A (en) * | 1987-12-28 | 1989-06-06 | Trustees Of Boston University | Rubbery, electrically non-conductive, and intrinsically magnetic graphite intercalation compounds and methods for their making |
US4987175A (en) * | 1988-11-21 | 1991-01-22 | Battelle Memorial Institute | Enhancement of the mechanical properties by graphite flake addition |
US5065948A (en) * | 1988-11-21 | 1991-11-19 | Battelle Memorial Institute | Apparatus for producing thin flakes |
US5019446A (en) * | 1988-11-21 | 1991-05-28 | Battelle Memorial Institute | Enhancement of mechanical properties of polymers by thin flake addition and apparatus for producing such thin flakes |
JPH02153812A (ja) * | 1988-12-06 | 1990-06-13 | Fuji Carbon Seizosho:Kk | 二種類以上の金属ハロゲン化物を同時に挿入させた黒鉛層間化合物、及び製造方法 |
JPH04170310A (ja) * | 1990-11-02 | 1992-06-18 | Alps Electric Co Ltd | 黒鉛層間化合物およびその製造方法 |
JPH04171605A (ja) * | 1990-11-02 | 1992-06-18 | Alps Electric Co Ltd | 導電性ペースト |
JP3434928B2 (ja) * | 1995-04-03 | 2003-08-11 | 科学技術振興事業団 | グラファイト層間化合物およびその製造方法 |
JP2009535294A (ja) * | 2006-05-01 | 2009-10-01 | 矢崎総業株式会社 | 炭素と非炭素との組織化されたアセンブリー、およびその製造方法 |
BRPI0703826A2 (pt) * | 2007-08-28 | 2009-04-28 | Nac De Grafite Ltda | bateria alcalina |
CN105655002B (zh) * | 2014-11-27 | 2017-06-23 | 松下知识产权经营株式会社 | 导电材料 |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2196293B1 (de) * | 1972-08-18 | 1975-03-07 | Armand Michel | |
US4565649A (en) * | 1974-08-23 | 1986-01-21 | Intercal Company | Graphite intercalation compounds |
GB1522808A (en) * | 1974-08-23 | 1978-08-31 | Vogel F L | Graphite intercalation compounds |
US4477374A (en) * | 1981-10-03 | 1984-10-16 | Central Glass Co., Ltd. | Ternary intercalation compound of a graphite with a metal fluoride and fluorine, a process for producing the same, and an electrically conductive material comprising the ternary intercalation compound |
US4604276A (en) * | 1983-09-19 | 1986-08-05 | Gte Laboratories Incorporated | Intercalation of small graphite flakes with a metal halide |
US4608192A (en) * | 1984-01-16 | 1986-08-26 | Gte Laboratories Incorporated | Graphite intercalates containing metal-charge transfer salts |
US4560409A (en) * | 1984-08-29 | 1985-12-24 | Superior Graphite | Metal bearing graphitic carbons |
-
1985
- 1985-08-17 JP JP60180046A patent/JPS6241706A/ja active Granted
-
1986
- 1986-08-05 US US06/893,259 patent/US4729884A/en not_active Expired - Fee Related
- 1986-08-13 EP EP86306249A patent/EP0212940B1/de not_active Expired - Lifetime
- 1986-08-13 DE DE8686306249T patent/DE3678360D1/de not_active Expired - Lifetime
Non-Patent Citations (3)
Title |
---|
CHEMICAL ABSTRACTS, vol. 92, no. 14, 7th April 1980, page 697, abstract no. 121021r, Columbus, Ohio, US; A.V. NEFED'EV et al.: "Synthesis, gamma-resonance spectra, and structure of laminar graphite compounds containing iron(III) chloride and molybdenum(V) chloride or iron(III) chloride and tungsten(VI) chloride", & ZH. STRUKT. KHIM. 1979, 20(5), 835-41 * |
CHEMICAL ABSTRACTS, vol. 95, no. 20, 16th November 1981, page 744, abstract no. 180084y, Columbus, Ohio, US; T. DZIEMIANOWICZ et al.: "Study of the system graphite-manganese(II) chloride-aluminum chloride", & EXT. ABSTR. PROGRAM-BIENN. CONF. CARBON 1981, 15th, 379-80 * |
MATERIALS SCIENCE AND ENGINEERING, vol. 31, 1977, pages 53-59, Elsevier Sequoia S.A., Lausanne, CH; E. STUMPP: "The intercalation of metal chlorides and bromides into graphite" * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0311298A2 (de) * | 1987-10-06 | 1989-04-12 | Cabotex Co. Ltd. | Verfahren zur Bereitung einer Einlagerungsverbindung Bereitung einer Einlagerungsverbindung |
EP0311298A3 (de) * | 1987-10-06 | 1992-01-08 | Cabotex Co. Ltd. | Verfahren zur Bereitung einer Einlagerungsverbindung Bereitung einer Einlagerungsverbindung |
EP0578887A1 (de) * | 1992-07-17 | 1994-01-19 | Inland Steel Company | Verfahren zur Herstellung von Einlagerungsverbindungen |
DE102021207914A1 (de) | 2020-12-15 | 2022-06-15 | Robert Bosch Gesellschaft mit beschränkter Haftung | Verfahren zum Herstellen eines elektrisch leitfähigen Leiterstrangs mit zumindest einem Kohlenstoffleiter |
WO2022128495A1 (de) | 2020-12-15 | 2022-06-23 | Robert Bosch Gmbh | Verfahren zum herstellen eines elektrisch leitfähigen leiterstrangs mit zumindest einem kohlenstoffleiter |
Also Published As
Publication number | Publication date |
---|---|
US4729884A (en) | 1988-03-08 |
EP0212940B1 (de) | 1991-03-27 |
EP0212940A3 (en) | 1988-03-16 |
DE3678360D1 (de) | 1991-05-02 |
JPS6241706A (ja) | 1987-02-23 |
JPS6362446B2 (de) | 1988-12-02 |
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